The site symmetry at the antimony in NaSbF6 has been examined by nuclear magnetic resonance. Antimony-123 resonance in polycrystalline NaSbF6 at 12.2 Mc. sec-1 and 19°C shows no second-order quadrupole effects. This is a reflection of a negligibly small or zero deformation fromOh symmetry of the surrounding atoms. Because of this and other considerations, NaSbF6 belongs to the space groupFm3m within the limits established by this work. Antimony-121 resonance in KSbF6, a compound for which the deformation fromOh symmetry is presumably known, exhibits a second order quadrupole effect which leads to a coupling constante2qQ/h of 6.1 ± 0.6 Mc. sec-1. A comparison of the data for the two compounds leands to an upper limit for the SbF-6 deformation of 7 × 10-4 rad in NaSbF6.